Preparation method and application of polycyclotriphosphazen porous material

A porous material, polycyclic phosphazene technology, applied in the field of preparation of polycyclic phosphazene porous materials, can solve the problems of lowering the ignition point of impregnated activated carbon, lower adsorption efficiency, secondary pollution, etc., and achieve good molecular thermal stability and low regeneration consumption The effect of low energy and mild reaction conditions

A porous material, polycyclic phosphazene technology, applied in the field of preparation of polycyclic phosphazene porous materials, can solve the problems of lowering the ignition point of impregnated activated carbon, lower adsorption efficiency, secondary pollution, etc., and achieve good molecular thermal stability and low regeneration consumption The effect of low energy and mild reaction conditions

CN106380604AInactive Publication Date: 2017-02-08CENT SOUTH UNIV
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  • Preparation method and application of polycyclotriphosphazen porous material
  • Preparation method and application of polycyclotriphosphazen porous material
  • Preparation method and application of polycyclotriphosphazen porous material

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Experimental program
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Effect test

Embodiment 1

[0033] Equipped with mechanical stirring, reflux condenser and constant pressure dropping funnel, thermometer, N 2 Into the 500mL five-neck round-bottomed flask of the introduction tube, add 300mL of acetonitrile, 3.47g (0.01mol) of hexachlorocyclotriphosphazene, and 5.16g (0.06mol) of piperazine in sequence, and after stirring evenly, slowly add 30mL of triethylamine dropwise, N 2 After reacting at 50°C for 24 hours under protection, the filtrate was removed by filtration, washed with water for 3 times and dried to obtain a cyclic phosphazene polymer. Finally, under vacuum conditions (0.1mmHg), heated to 200°C for 12 hours to obtain a polycyclic phosphine Nitrile porous material. After testing, the specific surface area of ​​the porous material is 1067m 2 / g, the average pore size is 2.1nm, CO 2 The adsorption capacity is 15.1 wt% (298K, 1 bar), and the adsorption capacity of iodine vapor is 90.5 wt% (333K).

Embodiment 2

[0035] Equipped with mechanical stirring, reflux condenser and constant pressure dropping funnel, thermometer, N 2 Into the 500mL five-necked round-bottomed flask with the introduction tube, add 250mL of tetrahydrofuran, 3.47g (0.01mol) of hexachlorocyclotriphosphazene, and 13.44g (0.08mol) of 4,4-dipiperidine in sequence. After stirring evenly, slowly add Pyridine 50mL, N 2 After reacting at 45°C for 48hrs under protection, the filtrate was removed by filtration, washed with water for 3 times and then dried to obtain a cyclic phosphazene polymer. Finally, under vacuum conditions (0.1mmHg), heated to 180°C for activation for 24hrs to obtain a polycyclic phosphazene porous material. After testing, the specific surface area of ​​the porous material is 1244m 2 / g, the average pore size is 1.8nm, CO 2 The adsorption amount is 17.3wt% (298K, 1bar), the iodine vapor adsorption amount is 102.1wt% (333K), and the iodine adsorption amount in n-hexane solution is 84mg / g (295K, 4hr) ...

Embodiment 3

[0037] Equipped with mechanical stirring, reflux condenser and constant pressure dropping funnel, thermometer, N 2 Into the 500mL five-neck round-bottomed flask of the introduction tube, add 400mL of acetone, 3.47g (0.01mol) of hexachlorocyclotriphosphazene, 1H,1'H-7,7'-bipyrimidine[4,5-b]pyridine 2.36g (0.1mol), after stirring evenly, slowly add lithium carbonate 5g, N 2 After reacting at 60°C for 12 hours under protection, remove the filtrate by filtration, wash with water for 3 times, and then dry to obtain the cyclic phosphazene polymer. Finally, under vacuum conditions (0.1mmHg), heat to 150°C for activation for 48 hours to obtain the polycyclic phosphazene porous material. After testing, the specific surface area of ​​the porous material is 1419m 2 / g, the average pore size is 1.6nm, CO 2 The adsorption capacity is 18.9wt% (273K, 1bar), CO 2 The adsorption capacity is 12.8 wt% (298K, 1 bar).

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Abstract

The invention discloses a preparation method and application of a polycyclotriphosphazen porous material, belonging to the field of functional polymer porous materials. The preparation method for the polycyclotriphosphazen porous material comprises the following steps: subjecting hexachlorocyclotriphosphazene monomer and a piperazine, pyrazine or pyrazole compound to a polycondensation and crosslinking reaction under the action of an acid binding agent; and then carrying out activation so as to obtain the porous material. The polycyclotriphosphazen porous material has the advantages of low cost, high specific surface area, capacity of regulating particle sizes in a large range at will, excellent stability and the like, is applied to a plurality of fields like catalyst carriers, gas capture and storage, in-depth treatment of metal ions and separation of radioactive pollutants, and especially has good capability in capturing micromolecules like iodine and iodomethane in CO2, iodine steam and solutions. The preparation method is simple and easily practicable in process, uses widely available raw materials and is especially suitable for industrial application.

Description

technical field [0001] The invention relates to a preparation method and application of a polycyclic phosphazene porous material, belonging to the field of functional polymer porous materials. Background technique [0002] Radioactive iodine is an important harmful nuclide produced by the nuclear industry, and it is also the main isotope used in medicine for diagnosis and treatment. In recent years, with the rapid development of the nuclear industry and the diagnosis and treatment industry, especially in accidental mines, radioactive iodine waste, including radioactive solids and radioactive gases, will inevitably be produced. Adsorption filtration is one of the methods commonly used in the nuclear industry to capture iodine, which has the advantages of high efficiency, low cost, and simple equipment. Porous materials and other physical adsorption of iodine have relatively more development prospects due to the characteristics of simple equipment operation, low energy consum...

Claims

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Application Information

Patent Timeline
08 Feb 2017
Publication
CN106380604A
IPC
C08G79/025; C08J9/00
CPC
C08G79/025; C08J9/00; C08J2385/02
Inventors
林益军; 喻桂朋